#------------------------------------------------------------------------------
#$Date: 2023-07-05 11:47:31 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/92/1569248.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1569248
loop_
_publ_author_name
'Shiels, Dominic'
'Pascual-Borràs, Magda'
'Waddell, Paul G.'
'Wills, Corinne'
'Poblet, Josep-Maria'
'Errington, R. John'
_publ_section_title
;
 A thirty-year old mystery solved: identification of a new heptatungstate
 from non-aqueous solutions.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7919
_journal_page_last               7922
_journal_paper_doi               10.1039/d3cc02061d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'O24 W7, 2(C2 H6 O S), 1.707(O), 5(C10 H16 N)'
_chemical_formula_sum            'C54 H92 N5 O27.71 S2 W7'
_chemical_formula_weight         2605.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-27 deposited with the CCDC.	2023-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7639(3)
_cell_length_b                   10.4977(2)
_cell_length_c                   29.5824(4)
_cell_measurement_reflns_used    29071
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      76.7480
_cell_measurement_theta_min      2.2040
_cell_volume                     7284.69(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00 -21.00   0.50    1.50    --  -92.01  71.00 -54.00  136
  2  ω    -72.00  21.00   0.50    1.50    --  -49.76  71.00 -54.00  186
  3  ω    -48.00 -18.00   0.50    1.50    --  -92.01  45.00 150.00   60
  4  ω     39.00  96.00   0.50    1.50    --  108.00 -95.00  30.00  114
  5  ω   -120.00 -78.00   0.50    1.50    --  -49.76-125.00-120.00   84
  6  ω   -168.00 -75.00   0.50    1.50    --  -92.01 -45.00-120.00  186
  7  ω   -153.00 -68.00   0.50    1.50    --  -92.01 -71.00 174.00  170
  8  ω    -93.00 -27.00   0.50    1.50    --  -49.76 -71.00 174.00  132
  9  ω     66.00 105.00   0.50    1.50    --  108.00 -77.00 -90.00   78
 10  ω     42.00  67.00   0.50    1.50    --  108.00 -61.00-150.00   50
 11  ω     23.00  71.00   0.50    1.50    --   96.11 -61.00 -30.00   96
 12  ω     18.00  43.00   0.50    1.50    --   96.11 -45.00-150.00   50
 13  ω     19.00  45.00   0.50    1.50    --   96.11 -45.00  30.00   52
 14  ω     19.00  50.00   0.50    1.50    --   96.11 -45.00-180.00   62
 15  ω     23.00  60.00   0.50    1.50    --   96.11 -61.00 120.00   74
 16  ω     39.00  64.00   0.50    1.50    --  108.00 -71.00 174.00   50
 17  ω     34.00  86.00   0.50    1.50    --   96.11 -71.00 174.00  104
 18  ω    -17.00  50.00   0.50    1.50    --   48.76 -71.00 174.00  134
 19  ω    111.00 137.00   0.50    1.50    --   96.11  71.00 -54.00   52
 20  ω    144.00 169.00   0.50    1.50    --  108.00  71.00 -54.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0598722000
_diffrn_orient_matrix_UB_12      0.0582695000
_diffrn_orient_matrix_UB_13      -0.0130172000
_diffrn_orient_matrix_UB_21      0.0148074000
_diffrn_orient_matrix_UB_22      0.1017115000
_diffrn_orient_matrix_UB_23      0.0376387000
_diffrn_orient_matrix_UB_31      0.0225622000
_diffrn_orient_matrix_UB_32      0.0883158000
_diffrn_orient_matrix_UB_33      -0.0345998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.391
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.044
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_description       block
_exptl_crystal_F_000             4891
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.151
_refine_diff_density_min         -2.735
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         14433
_refine_ls_number_restraints     960
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0408P)²+58.1946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11853
_reflns_number_total             14433
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc02061d2.cif
_cod_data_source_block           rje220110_fa
_cod_depositor_comments
'Adding full bibliography for 1569248--1569249.cif.'
_cod_database_code               1569248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H81 N5 W7 O24'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.321
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1A-O26A \\sim S1B-O26B
 with sigma of 0.02
 C54A-C53A \\sim C53B-C54B
 with sigma of 0.04
 S1A-C54A \\sim S1B-C53B
 with sigma of 0.02
 S1A-C53A \\sim S1B-C54B
 with sigma of 0.02
 O26A-C54A \\sim O26B-C53B
 with sigma of 0.04
 O26A-C53A \\sim O26B-C54B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1A \\sim O26A \\sim C53A \\sim C54A \\sim S1B \\sim O26B \\sim C53B \\sim
C54B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O28(0.70717) S1A(0.72599) O26A(0.72599) C53A(0.72599)
 H53A(0.72599) H53B(0.72599) H53C(0.72599) C54A(0.72599) H54A(0.72599)
 H54B(0.72599) H54C(0.72599) S1B(0.27401) O26B(0.27401) C53B(0.27401)
 H53D(0.27401) H53E(0.27401) H53F(0.27401) C54B(0.27401) H54D(0.27401)
 H54E(0.27401) H54F(0.27401)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C14(H14A,H14B), C24(H24A,H24B), C34(H34A,H34B), C44(H44A,H44B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53A(H53A,H53B,H53C), C54A(H54A,H54B,
 H54C), C53B(H53D,H53E,H53F), C54B(H54D,H54E,H54F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.595
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.37336(2) 0.78377(3) 0.50785(2) 0.02886(9) Uani 1 1 d . . . . .
W2 W 0.44051(2) 0.72155(3) 0.60285(2) 0.02717(8) Uani 1 1 d . . . . .
W3 W 0.32312(2) 0.48158(3) 0.56479(2) 0.02591(8) Uani 1 1 d . . . . .
W4 W 0.32839(2) 0.60972(3) 0.66520(2) 0.02557(8) Uani 1 1 d . . . . .
W5 W 0.23755(2) 0.82969(3) 0.62147(2) 0.02774(9) Uani 1 1 d . . . . .
W6 W 0.22811(2) 0.68928(3) 0.52089(2) 0.02816(8) Uani 1 1 d . . . . .
W7 W 0.20458(2) 0.52003(3) 0.60910(2) 0.02780(9) Uani 1 1 d . . . . .
S1 S 0.1440(3) 0.5514(6) 0.37259(13) 0.1271(19) Uani 1 1 d . . . . .
O1 O 0.4513(2) 0.7566(5) 0.53957(18) 0.0310(11) Uani 1 1 d . . . . .
O2 O 0.3802(2) 0.8627(5) 0.57459(17) 0.0292(11) Uani 1 1 d . . . . .
O3 O 0.3804(3) 0.9273(5) 0.48014(19) 0.0363(13) Uani 1 1 d . . . . .
O4 O 0.3727(2) 0.6732(5) 0.46318(18) 0.0357(13) Uani 1 1 d . . . . .
O5 O 0.4775(2) 0.5778(5) 0.61269(19) 0.0348(12) Uani 1 1 d . . . . .
O6 O 0.4897(2) 0.8266(5) 0.63262(19) 0.0335(12) Uani 1 1 d . . . . .
O7 O 0.3725(2) 0.6118(5) 0.55636(17) 0.0270(11) Uani 1 1 d . . . . .
O8 O 0.2926(2) 0.7869(5) 0.51150(17) 0.0315(11) Uani 1 1 d . . . . .
O9 O 0.2923(2) 0.9314(5) 0.61180(17) 0.0296(11) Uani 1 1 d . . . . .
O10 O 0.3886(2) 0.7058(5) 0.64691(17) 0.0270(10) Uani 1 1 d . . . . .
O11 O 0.3521(2) 0.3463(5) 0.54396(18) 0.0308(12) Uani 1 1 d . . . . .
O12 O 0.3594(2) 0.5693(5) 0.72011(17) 0.0289(11) Uani 1 1 d . . . . .
O13 O 0.1935(2) 0.9328(5) 0.64517(19) 0.0368(13) Uani 1 1 d . . . . .
O14 O 0.1864(3) 0.7140(6) 0.46870(19) 0.0399(13) Uani 1 1 d . . . . .
O15 O 0.3539(2) 0.4743(5) 0.62872(17) 0.0259(10) Uani 1 1 d . . . . .
O16 O 0.2841(2) 0.7533(5) 0.67537(17) 0.0272(11) Uani 1 1 d . . . . .
O17 O 0.2030(2) 0.8234(5) 0.55690(18) 0.0308(11) Uani 1 1 d . . . . .
O18 O 0.2725(2) 0.5421(5) 0.51124(16) 0.0290(11) Uani 1 1 d . . . . .
O19 O 0.2758(2) 0.6509(5) 0.59450(16) 0.0267(10) Uani 1 1 d . . . . .
O20 O 0.2546(2) 0.4059(5) 0.58247(17) 0.0286(11) Uani 1 1 d . . . . .
O21 O 0.2602(2) 0.5050(5) 0.66433(18) 0.0305(11) Uani 1 1 d . . . . .
O22 O 0.1824(2) 0.6760(5) 0.62909(18) 0.0320(12) Uani 1 1 d . . . . .
O23 O 0.1779(2) 0.5742(5) 0.54630(18) 0.0313(11) Uani 1 1 d . . . . .
O24 O 0.1524(2) 0.4148(6) 0.61926(19) 0.0372(13) Uani 1 1 d . . . . .
O25 O 0.1207(8) 0.4861(15) 0.3282(4) 0.177(7) Uani 1 1 d . . . . .
O27 O 0.2743(5) 0.6506(10) 0.3997(3) 0.094(3) Uani 1 1 d . . . . .
O28 O 0.0543(7) 0.2748(13) 0.3381(5) 0.100(5) Uani 0.7072 1 d . . P . .
N1 N 0.6211(3) 0.6659(7) 0.5781(2) 0.0330(14) Uani 1 1 d . . . . .
N2 N 0.4821(3) 1.1667(6) 0.5839(2) 0.0311(14) Uani 1 1 d . . . . .
N3 N 0.2823(3) 1.1909(6) 0.7153(2) 0.0324(14) Uani 1 1 d . . . . .
N4 N 0.1904(3) 0.1527(7) 0.5075(2) 0.0361(15) Uani 1 1 d . . . . .
N5 N -0.0075(4) -0.0035(8) 0.7490(3) 0.0520(19) Uani 1 1 d . . . . .
C1 C 0.5799(4) 0.6096(8) 0.5398(3) 0.0376(18) Uani 1 1 d . . . . .
H1A H 0.585948 0.517407 0.538667 0.056 Uiso 1 1 calc R U . . .
H1B H 0.585925 0.647949 0.510725 0.056 Uiso 1 1 calc R U . . .
H1C H 0.540823 0.626677 0.544808 0.056 Uiso 1 1 calc R U . . .
C2 C 0.6090(4) 0.8054(8) 0.5813(3) 0.041(2) Uani 1 1 d . . . . .
H2A H 0.613393 0.847082 0.552441 0.061 Uiso 1 1 calc R U . . .
H2B H 0.635788 0.843038 0.606400 0.061 Uiso 1 1 calc R U . . .
H2C H 0.569914 0.817424 0.587189 0.061 Uiso 1 1 calc R U . . .
C3 C 0.6807(4) 0.6475(11) 0.5691(3) 0.051(2) Uani 1 1 d . . . . .
H3A H 0.689867 0.556404 0.570070 0.076 Uiso 1 1 calc R U . . .
H3B H 0.707277 0.692275 0.592587 0.076 Uiso 1 1 calc R U . . .
H3C H 0.684066 0.681731 0.538870 0.076 Uiso 1 1 calc R U . . .
C4 C 0.6116(4) 0.5965(9) 0.6213(3) 0.0400(19) Uani 1 1 d . . . . .
H4A H 0.570651 0.602335 0.623926 0.048 Uiso 1 1 calc R U . . .
H4B H 0.620683 0.505309 0.618008 0.048 Uiso 1 1 calc R U . . .
C5 C 0.6459(4) 0.6450(9) 0.6652(3) 0.0429(19) Uani 1 1 d . . . . .
C6 C 0.6992(4) 0.5897(10) 0.6828(3) 0.050(2) Uani 1 1 d . . . . .
H6 H 0.715413 0.527749 0.665326 0.060 Uiso 1 1 calc R U . . .
C7 C 0.7272(5) 0.6251(12) 0.7246(4) 0.066(3) Uani 1 1 d . . . . .
H7 H 0.761902 0.583992 0.736860 0.079 Uiso 1 1 calc R U . . .
C8 C 0.7061(5) 0.7196(13) 0.7495(4) 0.065(3) Uani 1 1 d . . . . .
H8 H 0.726469 0.744055 0.778487 0.078 Uiso 1 1 calc R U . . .
C9 C 0.6554(5) 0.7787(13) 0.7325(4) 0.063(3) Uani 1 1 d . . . . .
H9 H 0.641232 0.845130 0.749366 0.076 Uiso 1 1 calc R U . . .
C10 C 0.6247(5) 0.7410(11) 0.6902(3) 0.052(2) Uani 1 1 d . . . . .
H10 H 0.589418 0.780819 0.678589 0.062 Uiso 1 1 calc R U . . .
C11 C 0.4550(4) 1.1120(8) 0.5390(3) 0.041(2) Uani 1 1 d . . . . .
H11A H 0.480321 1.124210 0.516302 0.061 Uiso 1 1 calc R U . . .
H11B H 0.418602 1.154987 0.528666 0.061 Uiso 1 1 calc R U . . .
H11C H 0.448231 1.020708 0.542672 0.061 Uiso 1 1 calc R U . . .
C12 C 0.4946(4) 1.3047(8) 0.5786(3) 0.0375(18) Uani 1 1 d . . . . .
H12A H 0.511280 1.340119 0.608402 0.056 Uiso 1 1 calc R U . . .
H12B H 0.459188 1.350003 0.566949 0.056 Uiso 1 1 calc R U . . .
H12C H 0.521568 1.314642 0.557015 0.056 Uiso 1 1 calc R U . . .
C13 C 0.4408(4) 1.1518(9) 0.6172(3) 0.043(2) Uani 1 1 d . . . . .
H13A H 0.429714 1.062112 0.618458 0.064 Uiso 1 1 calc R U . . .
H13B H 0.406868 1.203774 0.607080 0.064 Uiso 1 1 calc R U . . .
H13C H 0.458984 1.179731 0.647632 0.064 Uiso 1 1 calc R U . . .
C14 C 0.5357(4) 1.0897(8) 0.5992(3) 0.0365(17) Uani 1 1 d . . . . .
H14A H 0.524760 0.999808 0.603068 0.044 Uiso 1 1 calc R U . . .
H14B H 0.559551 1.092100 0.574640 0.044 Uiso 1 1 calc R U . . .
C15 C 0.5710(4) 1.1346(8) 0.6430(3) 0.0369(17) Uani 1 1 d . . . . .
C16 C 0.6146(4) 1.2220(10) 0.6420(3) 0.047(2) Uani 1 1 d . . . . .
H16 H 0.621348 1.254731 0.613394 0.056 Uiso 1 1 calc R U . . .
C17 C 0.6480(5) 1.2618(11) 0.6815(4) 0.058(3) Uani 1 1 d . . . . .
H17 H 0.678080 1.320794 0.680265 0.070 Uiso 1 1 calc R U . . .
C18 C 0.6377(5) 1.2151(11) 0.7232(4) 0.057(2) Uani 1 1 d . . . . .
H18 H 0.659752 1.244524 0.750868 0.068 Uiso 1 1 calc R U . . .
C19 C 0.5949(5) 1.1254(11) 0.7246(3) 0.058(2) Uani 1 1 d . . . . .
H19 H 0.588040 1.092536 0.753140 0.070 Uiso 1 1 calc R U . . .
C20 C 0.5628(4) 1.0847(10) 0.6845(3) 0.048(2) Uani 1 1 d . . . . .
H20 H 0.534595 1.021104 0.685443 0.057 Uiso 1 1 calc R U . . .
C21 C 0.2193(4) 1.2071(9) 0.7054(3) 0.044(2) Uani 1 1 d . . . . .
H21A H 0.210133 1.290721 0.691401 0.066 Uiso 1 1 calc R U . . .
H21B H 0.203535 1.201136 0.734010 0.066 Uiso 1 1 calc R U . . .
H21C H 0.202657 1.140179 0.684318 0.066 Uiso 1 1 calc R U . . .
C22 C 0.3055(4) 1.1993(8) 0.6706(3) 0.0373(19) Uani 1 1 d . . . . .
H22A H 0.292186 1.278292 0.654697 0.056 Uiso 1 1 calc R U . . .
H22B H 0.292018 1.126152 0.651250 0.056 Uiso 1 1 calc R U . . .
H22C H 0.347256 1.198922 0.676821 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3078(4) 1.2957(8) 0.7460(3) 0.0395(19) Uani 1 1 d . . . . .
H23A H 0.349460 1.291770 0.749178 0.059 Uiso 1 1 calc R U . . .
H23B H 0.296247 1.286319 0.776136 0.059 Uiso 1 1 calc R U . . .
H23C H 0.294463 1.377999 0.732709 0.059 Uiso 1 1 calc R U . . .
C24 C 0.2953(4) 1.0623(8) 0.7378(3) 0.0347(17) Uani 1 1 d . . . . .
H24A H 0.278730 1.059737 0.766385 0.042 Uiso 1 1 calc R U . . .
H24B H 0.276151 0.995713 0.717120 0.042 Uiso 1 1 calc R U . . .
C25 C 0.3578(4) 1.0302(8) 0.7490(3) 0.0341(16) Uani 1 1 d . . . . .
C26 C 0.3839(4) 0.9626(8) 0.7172(3) 0.0356(17) Uani 1 1 d . . . . .
H26 H 0.362363 0.937990 0.688673 0.043 Uiso 1 1 calc R U . . .
C27 C 0.4411(4) 0.9317(9) 0.7274(3) 0.047(2) Uani 1 1 d . . . . .
H27 H 0.458712 0.885413 0.705869 0.057 Uiso 1 1 calc R U . . .
C28 C 0.4727(4) 0.9674(11) 0.7685(3) 0.053(2) Uani 1 1 d . . . . .
H28 H 0.512110 0.947348 0.775177 0.064 Uiso 1 1 calc R U . . .
C29 C 0.4465(5) 1.0331(11) 0.8002(3) 0.054(2) Uani 1 1 d . . . . .
H29 H 0.468157 1.056161 0.828851 0.065 Uiso 1 1 calc R U . . .
C30 C 0.3904(4) 1.0651(10) 0.7910(3) 0.045(2) Uani 1 1 d . . . . .
H30 H 0.373264 1.110977 0.812938 0.054 Uiso 1 1 calc R U . . .
C31 C 0.1583(4) 0.1434(9) 0.5474(3) 0.047(2) Uani 1 1 d . . . . .
H31A H 0.118091 0.164324 0.537073 0.070 Uiso 1 1 calc R U . . .
H31B H 0.174573 0.203354 0.571330 0.070 Uiso 1 1 calc R U . . .
H31C H 0.161297 0.056502 0.559622 0.070 Uiso 1 1 calc R U . . .
C32 C 0.1837(4) 0.2853(8) 0.4896(3) 0.042(2) Uani 1 1 d . . . . .
H32A H 0.205458 0.295477 0.464325 0.063 Uiso 1 1 calc R U . . .
H32B H 0.197946 0.345428 0.514122 0.063 Uiso 1 1 calc R U . . .
H32C H 0.143314 0.302405 0.478520 0.063 Uiso 1 1 calc R U . . .
C33 C 0.2526(4) 0.1273(9) 0.5249(3) 0.045(2) Uani 1 1 d . . . . .
H33A H 0.257298 0.039138 0.535709 0.068 Uiso 1 1 calc R U . . .
H33B H 0.266109 0.185597 0.550129 0.068 Uiso 1 1 calc R U . . .
H33C H 0.274688 0.140596 0.499995 0.068 Uiso 1 1 calc R U . . .
C34 C 0.1652(4) 0.0568(8) 0.4717(3) 0.0393(18) Uani 1 1 d . . . . .
H34A H 0.123888 0.073521 0.463237 0.047 Uiso 1 1 calc R U . . .
H34B H 0.169805 -0.029748 0.485070 0.047 Uiso 1 1 calc R U . . .
C35 C 0.1925(4) 0.0605(9) 0.4288(3) 0.0407(18) Uani 1 1 d . . . . .
C36 C 0.1687(5) 0.1403(11) 0.3928(3) 0.057(2) Uani 1 1 d . . . . .
H36 H 0.136235 0.190508 0.395667 0.068 Uiso 1 1 calc R U . . .
C37 C 0.1927(6) 0.1460(13) 0.3530(4) 0.070(3) Uani 1 1 d . . . . .
H37 H 0.177426 0.201767 0.328857 0.084 Uiso 1 1 calc R U . . .
C38 C 0.2390(6) 0.0698(13) 0.3489(4) 0.070(3) Uani 1 1 d . . . . .
H38 H 0.255395 0.072989 0.321668 0.084 Uiso 1 1 calc R U . . .
C39 C 0.2617(5) -0.0108(11) 0.3839(4) 0.063(3) Uani 1 1 d . . . . .
H39 H 0.293529 -0.062741 0.380681 0.075 Uiso 1 1 calc R U . . .
C40 C 0.2380(4) -0.0166(9) 0.4241(4) 0.050(2) Uani 1 1 d . . . . .
H40 H 0.253238 -0.073186 0.448061 0.061 Uiso 1 1 calc R U . . .
C41 C 0.0120(6) -0.0913(12) 0.7890(4) 0.075(4) Uani 1 1 d . . . . .
H41A H 0.051877 -0.072916 0.801595 0.113 Uiso 1 1 calc R U . . .
H41B H 0.008602 -0.179996 0.778565 0.113 Uiso 1 1 calc R U . . .
H41C H -0.011803 -0.077969 0.812737 0.113 Uiso 1 1 calc R U . . .
C42 C -0.0693(5) -0.0198(13) 0.7317(4) 0.069(3) Uani 1 1 d . . . . .
H42A H -0.090901 -0.010177 0.757091 0.104 Uiso 1 1 calc R U . . .
H42B H -0.076081 -0.104826 0.718250 0.104 Uiso 1 1 calc R U . . .
H42C H -0.081779 0.044868 0.708338 0.104 Uiso 1 1 calc R U . . .
C43 C 0.0041(4) 0.1312(10) 0.7645(3) 0.049(2) Uani 1 1 d . . . . .
H43A H 0.045154 0.142723 0.774407 0.073 Uiso 1 1 calc R U . . .
H43B H -0.016171 0.149616 0.790098 0.073 Uiso 1 1 calc R U . . .
H43C H -0.009073 0.189364 0.739089 0.073 Uiso 1 1 calc R U . . .
C44 C 0.0268(5) -0.0391(10) 0.7121(3) 0.054(2) Uani 1 1 d . . . . .
H44A H 0.067652 -0.039023 0.725656 0.065 Uiso 1 1 calc R U . . .
H44B H 0.016567 -0.127228 0.702055 0.065 Uiso 1 1 calc R U . . .
C45 C 0.0190(5) 0.0457(11) 0.6705(4) 0.060(3) Uani 1 1 d . . . . .
C46 C -0.0255(7) 0.0258(14) 0.6342(4) 0.089(5) Uani 1 1 d . . . . .
H46 H -0.053083 -0.038767 0.635904 0.107 Uiso 1 1 calc R U . . .
C47 C -0.0284(8) 0.1022(16) 0.5956(5) 0.110(6) Uani 1 1 d . . . . .
H47 H -0.057502 0.087339 0.570096 0.132 Uiso 1 1 calc R U . . .
C48 C 0.0097(7) 0.1982(15) 0.5936(5) 0.091(5) Uani 1 1 d . . . . .
H48 H 0.006399 0.250703 0.567174 0.109 Uiso 1 1 calc R U . . .
C49 C 0.0516(6) 0.2191(12) 0.6287(4) 0.075(3) Uani 1 1 d . . . . .
H49 H 0.078184 0.285732 0.626786 0.090 Uiso 1 1 calc R U . . .
C50 C 0.0567(5) 0.1452(12) 0.6674(4) 0.062(3) Uani 1 1 d . . . . .
H50 H 0.086277 0.162189 0.692251 0.074 Uiso 1 1 calc R U . . .
C51 C 0.0915(8) 0.5368(18) 0.4080(6) 0.123(6) Uani 1 1 d . . . . .
H51A H 0.055719 0.574036 0.392530 0.184 Uiso 1 1 calc R U . . .
H51B H 0.103966 0.581617 0.436885 0.184 Uiso 1 1 calc R U . . .
H51C H 0.085558 0.446471 0.414184 0.184 Uiso 1 1 calc R U . . .
C52 C 0.1384(11) 0.7167(18) 0.3595(5) 0.150(9) Uani 1 1 d . . . . .
H52A H 0.167777 0.740492 0.341291 0.224 Uiso 1 1 calc R U . . .
H52B H 0.143731 0.765991 0.388010 0.224 Uiso 1 1 calc R U . . .
H52C H 0.100636 0.734688 0.342030 0.224 Uiso 1 1 calc R U . . .
S1A S -0.0120(2) 0.2565(7) 0.4566(2) 0.0881(16) Uani 0.726 1 d D U P A 1
O26A O 0.0396(5) 0.2486(17) 0.4317(6) 0.089(4) Uani 0.726 1 d D U P A 1
C53A C -0.0667(8) 0.168(2) 0.4207(9) 0.102(6) Uani 0.726 1 d D U P A 1
H53A H -0.070573 0.199146 0.389185 0.153 Uiso 0.726 1 calc R U P A 1
H53B H -0.103032 0.177908 0.431993 0.153 Uiso 0.726 1 calc R U P A 1
H53C H -0.056308 0.077138 0.421416 0.153 Uiso 0.726 1 calc R U P A 1
C54A C -0.0449(8) 0.409(2) 0.4397(8) 0.089(6) Uani 0.726 1 d D U P A 1
H54A H -0.018238 0.477613 0.450524 0.134 Uiso 0.726 1 calc R U P A 1
H54B H -0.079648 0.418429 0.453314 0.134 Uiso 0.726 1 calc R U P A 1
H54C H -0.054514 0.412502 0.406297 0.134 Uiso 0.726 1 calc R U P A 1
S1B S -0.0138(6) 0.2665(17) 0.4269(6) 0.094(4) Uani 0.274 1 d D U P B 2
O26B O 0.0425(11) 0.228(4) 0.4583(14) 0.087(9) Uani 0.274 1 d D U P B 2
C53B C -0.0623(18) 0.165(5) 0.454(2) 0.097(10) Uani 0.274 1 d D U P B 2
H53D H -0.055914 0.179411 0.486939 0.145 Uiso 0.274 1 calc R U P B 2
H53E H -0.054891 0.075110 0.447624 0.145 Uiso 0.274 1 calc R U P B 2
H53F H -0.101870 0.185645 0.441110 0.145 Uiso 0.274 1 calc R U P B 2
C54B C -0.033(2) 0.406(4) 0.4568(19) 0.088(10) Uani 0.274 1 d D U P B 2
H54D H -0.035485 0.383873 0.488538 0.131 Uiso 0.274 1 calc R U P B 2
H54E H -0.069351 0.439365 0.441551 0.131 Uiso 0.274 1 calc R U P B 2
H54F H -0.003195 0.471670 0.456630 0.131 Uiso 0.274 1 calc R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -1 0.0109
1 0 1 0.0079
0 1 -1 0.0272
0 -1 1 0.0242
1 0 -1 0.0303
-1 0 1 0.0143
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 W2 38.52(14) . . ?
O1 W1 O2 71.7(2) . . ?
O1 W1 O7 71.94(19) . . ?
O2 W1 W2 44.05(14) . . ?
O2 W1 O7 74.58(18) . . ?
O3 W1 W2 122.8(2) . . ?
O3 W1 O1 101.4(3) . . ?
O3 W1 O2 95.8(2) . . ?
O3 W1 O4 102.0(3) . . ?
O3 W1 O7 169.5(2) . . ?
O3 W1 O8 100.6(2) . . ?
O4 W1 W2 119.24(19) . . ?
O4 W1 O1 99.1(2) . . ?
O4 W1 O2 161.3(2) . . ?
O4 W1 O7 87.2(2) . . ?
O4 W1 O8 99.4(2) . . ?
O7 W1 W2 47.15(13) . . ?
O8 W1 W2 109.05(15) . . ?
O8 W1 O1 147.6(2) . . ?
O8 W1 O2 82.6(2) . . ?
O8 W1 O7 82.6(2) . . ?
O1 W2 W1 38.39(16) . . ?
O1 W2 O2 71.3(2) . . ?
O1 W2 O7 72.9(2) . . ?
O2 W2 W1 43.69(13) . . ?
O2 W2 O7 75.3(2) . . ?
O5 W2 W1 120.66(19) . . ?
O5 W2 O1 100.5(2) . . ?
O5 W2 O2 162.2(2) . . ?
O5 W2 O7 87.3(2) . . ?
O5 W2 O10 99.9(2) . . ?
O6 W2 W1 122.46(18) . . ?
O6 W2 O1 100.6(2) . . ?
O6 W2 O2 96.5(2) . . ?
O6 W2 O5 100.6(3) . . ?
O6 W2 O7 170.7(2) . . ?
O6 W2 O10 99.3(2) . . ?
O7 W2 W1 48.40(13) . . ?
O10 W2 W1 109.87(15) . . ?
O10 W2 O1 148.2(2) . . ?
O10 W2 O2 82.1(2) . . ?
O10 W2 O7 84.03(19) . . ?
O7 W3 O15 90.7(2) . . ?
O7 W3 O18 88.4(2) . . ?
O7 W3 O19 80.95(19) . . ?
O7 W3 O20 155.7(2) . . ?
O11 W3 O7 105.2(2) . . ?
O11 W3 O15 102.0(2) . . ?
O11 W3 O18 102.0(2) . . ?
O11 W3 O19 173.8(2) . . ?
O11 W3 O20 99.0(2) . . ?
O15 W3 O18 155.4(2) . . ?
O15 W3 O19 77.94(18) . . ?
O15 W3 O20 85.6(2) . . ?
O18 W3 O19 77.62(19) . . ?
O18 W3 O20 85.2(2) . . ?
O20 W3 O19 74.82(19) . . ?
O10 W4 O15 85.1(2) . . ?
O10 W4 O19 88.1(2) . . ?
O10 W4 O21 162.9(2) . . ?
O12 W4 O10 99.8(2) . . ?
O12 W4 O15 102.7(2) . . ?
O12 W4 O16 102.2(2) . . ?
O12 W4 O19 172.1(2) . . ?
O12 W4 O21 95.9(2) . . ?
O15 W4 O19 78.7(2) . . ?
O15 W4 O21 85.0(2) . . ?
O16 W4 O10 94.9(2) . . ?
O16 W4 O15 154.8(2) . . ?
O16 W4 O19 76.1(2) . . ?
O16 W4 O21 88.2(2) . . ?
O21 W4 O19 76.4(2) . . ?
O9 W5 O16 92.6(2) . . ?
O9 W5 O17 93.9(2) . . ?
O9 W5 O19 95.6(2) . . ?
O9 W5 O22 167.9(2) . . ?
O13 W5 O9 101.5(3) . . ?
O13 W5 O16 103.0(2) . . ?
O13 W5 O17 103.3(2) . . ?
O13 W5 O19 162.9(2) . . ?
O13 W5 O22 90.5(2) . . ?
O16 W5 O19 75.14(19) . . ?
O16 W5 O22 83.1(2) . . ?
O17 W5 O16 151.0(2) . . ?
O17 W5 O19 76.1(2) . . ?
O17 W5 O22 84.7(2) . . ?
O22 W5 O19 72.41(19) . . ?
O8 W6 O17 90.9(2) . . ?
O8 W6 O18 86.4(2) . . ?
O8 W6 O19 87.0(2) . . ?
O8 W6 O23 163.0(2) . . ?
O14 W6 O8 98.7(3) . . ?
O14 W6 O17 101.7(3) . . ?
O14 W6 O18 103.9(3) . . ?
O14 W6 O19 173.9(2) . . ?
O14 W6 O23 98.1(3) . . ?
O17 W6 O19 75.8(2) . . ?
O17 W6 O23 88.6(2) . . ?
O18 W6 O17 154.4(2) . . ?
O18 W6 O19 78.61(19) . . ?
O18 W6 O23 86.7(2) . . ?
O23 W6 O19 76.4(2) . . ?
O20 W7 O19 76.9(2) . . ?
O20 W7 O23 85.4(2) . . ?
O21 W7 O19 77.3(2) . . ?
O21 W7 O20 85.0(2) . . ?
O21 W7 O23 154.4(2) . . ?
O22 W7 O19 77.5(2) . . ?
O22 W7 O20 154.4(2) . . ?
O22 W7 O21 89.6(2) . . ?
O22 W7 O23 88.9(2) . . ?
O23 W7 O19 77.4(2) . . ?
O24 W7 O19 177.3(2) . . ?
O24 W7 O20 100.4(2) . . ?
O24 W7 O21 102.4(2) . . ?
O24 W7 O22 105.2(3) . . ?
O24 W7 O23 102.7(2) . . ?
O25 S1 C51 106.4(9) . . ?
O25 S1 C52 104.5(9) . . ?
C51 S1 C52 100.3(11) . . ?
W1 O1 W2 103.1(2) . . ?
W1 O2 W2 92.3(2) . . ?
W2 O7 W1 84.45(17) . . ?
W3 O7 W1 137.1(3) . . ?
W3 O7 W2 134.7(3) . . ?
W6 O8 W1 145.8(3) . . ?
W4 O10 W2 145.7(3) . . ?
W3 O15 W4 114.6(2) . . ?
W4 O16 W5 116.9(2) . . ?
W6 O17 W5 116.6(3) . . ?
W6 O18 W3 115.3(2) . . ?
W4 O19 W3 88.56(18) . . ?
W4 O19 W6 176.1(2) . . ?
W5 O19 W3 173.7(2) . . ?
W5 O19 W4 91.46(17) . . ?
W5 O19 W6 91.32(18) . . ?
W6 O19 W3 88.37(16) . . ?
W7 O19 W3 91.70(18) . . ?
W7 O19 W4 91.52(17) . . ?
W7 O19 W5 94.62(18) . . ?
W7 O19 W6 90.97(18) . . ?
W7 O20 W3 116.6(3) . . ?
W7 O21 W4 114.7(2) . . ?
W7 O22 W5 115.4(3) . . ?
W6 O23 W7 115.2(3) . . ?
C1 N1 C2 108.9(7) . . ?
C1 N1 C4 106.4(6) . . ?
C2 N1 C4 111.1(6) . . ?
C3 N1 C1 109.7(7) . . ?
C3 N1 C2 109.5(7) . . ?
C3 N1 C4 111.1(7) . . ?
C11 N2 C13 107.9(7) . . ?
C11 N2 C14 106.4(6) . . ?
C12 N2 C11 110.3(6) . . ?
C12 N2 C13 109.3(6) . . ?
C12 N2 C14 112.2(6) . . ?
C13 N2 C14 110.7(6) . . ?
C21 N3 C22 108.4(7) . . ?
C21 N3 C23 109.5(7) . . ?
C21 N3 C24 108.4(6) . . ?
C23 N3 C22 108.6(6) . . ?
C23 N3 C24 110.9(7) . . ?
C24 N3 C22 111.0(6) . . ?
C31 N4 C33 108.3(7) . . ?
C31 N4 C34 108.1(7) . . ?
C32 N4 C31 107.5(7) . . ?
C32 N4 C33 109.3(7) . . ?
C32 N4 C34 111.4(7) . . ?
C33 N4 C34 112.1(7) . . ?
C42 N5 C41 111.2(9) . . ?
C42 N5 C43 109.7(9) . . ?
C42 N5 C44 109.8(8) . . ?
C43 N5 C41 108.6(8) . . ?
C43 N5 C44 111.2(8) . . ?
C44 N5 C41 106.4(9) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 108.4 . . ?
N1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C5 C4 N1 115.5(7) . . ?
C5 C4 H4A 108.4 . . ?
C5 C4 H4B 108.4 . . ?
C6 C5 C4 120.5(9) . . ?
C10 C5 C4 120.7(8) . . ?
C10 C5 C6 118.8(9) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.1(11) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.1(11) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.1(11) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0(12) . . ?
C10 C9 H9 120.0 . . ?
C5 C10 C9 119.9(10) . . ?
C5 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14A 108.6 . . ?
N2 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 N2 114.6(7) . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C16 C15 C14 120.2(8) . . ?
C20 C15 C14 120.8(8) . . ?
C20 C15 C16 118.8(9) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 C15 121.1(9) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 120.3 . . ?
C16 C17 C18 119.4(11) . . ?
C18 C17 H17 120.3 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0(10) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.6(10) . . ?
C20 C19 H19 120.2 . . ?
C15 C20 H20 119.5 . . ?
C19 C20 C15 121.0(10) . . ?
C19 C20 H20 119.5 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 H24A 108.5 . . ?
N3 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C25 C24 N3 114.9(7) . . ?
C25 C24 H24A 108.5 . . ?
C25 C24 H24B 108.5 . . ?
C26 C25 C24 119.5(8) . . ?
C26 C25 C30 119.1(8) . . ?
C30 C25 C24 121.5(7) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.9(8) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.5(9) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.3 . . ?
C27 C28 C29 119.5(9) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 119.4 . . ?
C30 C29 C28 121.2(10) . . ?
C30 C29 H29 119.4 . . ?
C25 C30 H30 120.1 . . ?
C29 C30 C25 119.8(8) . . ?
C29 C30 H30 120.1 . . ?
N4 C31 H31A 109.5 . . ?
N4 C31 H31B 109.5 . . ?
N4 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C32 H32A 109.5 . . ?
N4 C32 H32B 109.5 . . ?
N4 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 H33A 109.5 . . ?
N4 C33 H33B 109.5 . . ?
N4 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 H34A 108.9 . . ?
N4 C34 H34B 108.9 . . ?
N4 C34 C35 113.3(7) . . ?
H34A C34 H34B 107.7 . . ?
C35 C34 H34A 108.9 . . ?
C35 C34 H34B 108.9 . . ?
C36 C35 C34 118.5(9) . . ?
C40 C35 C34 121.1(9) . . ?
C40 C35 C36 120.3(9) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 120.0(11) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 H37 120.3 . . ?
C38 C37 C36 119.3(12) . . ?
C38 C37 H37 120.3 . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.7(11) . . ?
C39 C38 H38 119.7 . . ?
C38 C39 H39 119.8 . . ?
C38 C39 C40 120.3(12) . . ?
C40 C39 H39 119.8 . . ?
C35 C40 C39 119.3(10) . . ?
C35 C40 H40 120.3 . . ?
C39 C40 H40 120.3 . . ?
N5 C41 H41A 109.5 . . ?
N5 C41 H41B 109.5 . . ?
N5 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N5 C42 H42A 109.5 . . ?
N5 C42 H42B 109.5 . . ?
N5 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 H43A 109.5 . . ?
N5 C43 H43B 109.5 . . ?
N5 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N5 C44 H44A 108.3 . . ?
N5 C44 H44B 108.3 . . ?
H44A C44 H44B 107.4 . . ?
C45 C44 N5 115.7(9) . . ?
C45 C44 H44A 108.3 . . ?
C45 C44 H44B 108.3 . . ?
C46 C45 C44 121.3(10) . . ?
C50 C45 C44 120.2(10) . . ?
C50 C45 C46 118.6(11) . . ?
C45 C46 H46 120.7 . . ?
C47 C46 C45 118.6(12) . . ?
C47 C46 H46 120.7 . . ?
C46 C47 H47 119.5 . . ?
C48 C47 C46 121.0(13) . . ?
C48 C47 H47 119.5 . . ?
C47 C48 H48 119.8 . . ?
C49 C48 C47 120.5(13) . . ?
C49 C48 H48 119.8 . . ?
C48 C49 H49 119.7 . . ?
C48 C49 C50 120.6(11) . . ?
C50 C49 H49 119.7 . . ?
C45 C50 H50 119.7 . . ?
C49 C50 C45 120.6(11) . . ?
C49 C50 H50 119.7 . . ?
S1 C51 H51A 109.5 . . ?
S1 C51 H51B 109.5 . . ?
S1 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
S1 C52 H52A 109.5 . . ?
S1 C52 H52B 109.5 . . ?
S1 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O26A S1A C53A 104.3(10) . . ?
O26A S1A C54A 105.0(10) . . ?
C53A S1A C54A 93.3(10) . . ?
S1A C53A H53A 109.5 . . ?
S1A C53A H53B 109.5 . . ?
S1A C53A H53C 109.5 . . ?
H53A C53A H53B 109.5 . . ?
H53A C53A H53C 109.5 . . ?
H53B C53A H53C 109.5 . . ?
S1A C54A H54A 109.5 . . ?
S1A C54A H54B 109.5 . . ?
S1A C54A H54C 109.5 . . ?
H54A C54A H54B 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
O26B S1B C53B 97.4(19) . . ?
O26B S1B C54B 100(2) . . ?
C54B S1B C53B 92.3(18) . . ?
S1B C53B H53D 109.5 . . ?
S1B C53B H53E 109.5 . . ?
S1B C53B H53F 109.5 . . ?
H53D C53B H53E 109.5 . . ?
H53D C53B H53F 109.5 . . ?
H53E C53B H53F 109.5 . . ?
S1B C54B H54D 109.5 . . ?
S1B C54B H54E 109.5 . . ?
S1B C54B H54F 109.5 . . ?
H54D C54B H54E 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 W2 3.0718(5) . ?
W1 O1 1.958(6) . ?
W1 O2 2.124(5) . ?
W1 O3 1.736(6) . ?
W1 O4 1.757(5) . ?
W1 O7 2.308(5) . ?
W1 O8 1.939(6) . ?
W2 O1 1.964(5) . ?
W2 O2 2.138(5) . ?
W2 O5 1.748(6) . ?
W2 O6 1.740(6) . ?
W2 O7 2.263(5) . ?
W2 O10 1.939(5) . ?
W3 O7 1.844(5) . ?
W3 O11 1.733(5) . ?
W3 O15 1.917(5) . ?
W3 O18 1.937(5) . ?
W3 O19 2.348(5) . ?
W3 O20 1.956(5) . ?
W4 O10 1.900(5) . ?
W4 O12 1.726(5) . ?
W4 O15 1.940(5) . ?
W4 O16 1.890(5) . ?
W4 O19 2.299(5) . ?
W4 O21 1.954(5) . ?
W5 O9 1.741(5) . ?
W5 O13 1.730(5) . ?
W5 O16 1.961(5) . ?
W5 O17 1.956(5) . ?
W5 O19 2.284(5) . ?
W5 O22 2.113(5) . ?
W6 O8 1.901(5) . ?
W6 O14 1.716(6) . ?
W6 O17 1.918(5) . ?
W6 O18 1.917(5) . ?
W6 O19 2.324(5) . ?
W6 O23 1.933(5) . ?
W7 O19 2.274(5) . ?
W7 O20 1.942(5) . ?
W7 O21 1.937(6) . ?
W7 O22 1.846(5) . ?
W7 O23 1.949(5) . ?
W7 O24 1.723(6) . ?
S1 O25 1.506(12) . ?
S1 C51 1.759(19) . ?
S1 C52 1.778(19) . ?
N1 C1 1.497(11) . ?
N1 C2 1.499(11) . ?
N1 C3 1.495(11) . ?
N1 C4 1.519(10) . ?
N2 C11 1.494(10) . ?
N2 C12 1.492(10) . ?
N2 C13 1.506(10) . ?
N2 C14 1.517(11) . ?
N3 C21 1.490(11) . ?
N3 C22 1.516(9) . ?
N3 C23 1.491(11) . ?
N3 C24 1.514(10) . ?
N4 C31 1.507(11) . ?
N4 C32 1.490(11) . ?
N4 C33 1.507(11) . ?
N4 C34 1.514(10) . ?
N5 C41 1.513(13) . ?
N5 C42 1.487(14) . ?
N5 C43 1.498(13) . ?
N5 C44 1.509(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.506(13) . ?
C5 C6 1.414(13) . ?
C5 C10 1.391(14) . ?
C6 H6 0.9500 . ?
C6 C7 1.360(15) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(17) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.401(15) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.503(12) . ?
C15 C16 1.389(13) . ?
C15 C20 1.377(12) . ?
C16 H16 0.9500 . ?
C16 C17 1.368(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(15) . ?
C18 H18 0.9500 . ?
C18 C19 1.390(16) . ?
C19 H19 0.9500 . ?
C19 C20 1.371(14) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.506(12) . ?
C25 C26 1.400(11) . ?
C25 C30 1.403(12) . ?
C26 H26 0.9500 . ?
C26 C27 1.383(13) . ?
C27 H27 0.9500 . ?
C27 C28 1.374(14) . ?
C28 H28 0.9500 . ?
C28 C29 1.389(14) . ?
C29 H29 0.9500 . ?
C29 C30 1.359(13) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.515(12) . ?
C35 C36 1.400(13) . ?
C35 C40 1.375(14) . ?
C36 H36 0.9500 . ?
C36 C37 1.390(15) . ?
C37 H37 0.9500 . ?
C37 C38 1.381(18) . ?
C38 H38 0.9500 . ?
C38 C39 1.379(17) . ?
C39 H39 0.9500 . ?
C39 C40 1.395(14) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.506(15) . ?
C45 C46 1.396(16) . ?
C45 C50 1.389(15) . ?
C46 H46 0.9500 . ?
C46 C47 1.390(18) . ?
C47 H47 0.9500 . ?
C47 C48 1.362(18) . ?
C48 H48 0.9500 . ?
C48 C49 1.336(18) . ?
C49 H49 0.9500 . ?
C49 C50 1.372(17) . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
S1A O26A 1.530(13) . ?
S1A C53A 1.80(2) . ?
S1A C54A 1.81(2) . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A H53C 0.9800 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
S1B O26B 1.555(19) . ?
S1B C53B 1.84(3) . ?
S1B C54B 1.81(3) . ?
C53B H53D 0.9800 . ?
C53B H53E 0.9800 . ?
C53B H53F 0.9800 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 W4 O16 W5 81.2(3) . . . . ?
O11 W3 O7 W1 106.3(4) . . . . ?
O11 W3 O7 W2 -103.8(4) . . . . ?
O12 W4 O10 W2 121.6(5) . . . . ?
O12 W4 O16 W5 -177.6(3) . . . . ?
O15 W3 O7 W1 -151.1(4) . . . . ?
O15 W3 O7 W2 -1.1(4) . . . . ?
O15 W4 O10 W2 19.5(5) . . . . ?
O15 W4 O16 W5 -7.7(7) . . . . ?
O16 W4 O10 W2 -135.2(5) . . . . ?
O18 W3 O7 W1 4.3(4) . . . . ?
O18 W3 O7 W2 154.2(4) . . . . ?
O19 W3 O7 W1 -73.5(3) . . . . ?
O19 W3 O7 W2 76.5(3) . . . . ?
O19 W4 O10 W2 -59.3(5) . . . . ?
O19 W4 O16 W5 -5.5(2) . . . . ?
O19 W7 O22 W5 0.3(2) . . . . ?
O20 W3 O7 W1 -70.4(7) . . . . ?
O20 W3 O7 W2 79.6(7) . . . . ?
O20 W7 O22 W5 0.0(7) . . . . ?
O21 W4 O10 W2 -35.0(11) . . . . ?
O21 W4 O16 W5 -81.9(3) . . . . ?
O21 W7 O22 W5 77.4(3) . . . . ?
O23 W7 O22 W5 -77.0(3) . . . . ?
O24 W7 O22 W5 -179.8(3) . . . . ?
N1 C4 C5 C6 -93.1(10) . . . . ?
N1 C4 C5 C10 89.7(10) . . . . ?
N2 C14 C15 C16 -91.9(10) . . . . ?
N2 C14 C15 C20 91.9(10) . . . . ?
N3 C24 C25 C26 -92.3(9) . . . . ?
N3 C24 C25 C30 88.6(9) . . . . ?
N4 C34 C35 C36 -90.8(10) . . . . ?
N4 C34 C35 C40 92.0(10) . . . . ?
N5 C44 C45 C46 -85.5(14) . . . . ?
N5 C44 C45 C50 95.3(13) . . . . ?
C1 N1 C4 C5 -175.6(7) . . . . ?
C2 N1 C4 C5 -57.2(10) . . . . ?
C3 N1 C4 C5 65.0(10) . . . . ?
C4 C5 C6 C7 -173.4(9) . . . . ?
C4 C5 C10 C9 175.6(9) . . . . ?
C5 C6 C7 C8 -3.5(16) . . . . ?
C6 C5 C10 C9 -1.6(14) . . . . ?
C6 C7 C8 C9 0.9(18) . . . . ?
C7 C8 C9 C10 1.3(18) . . . . ?
C8 C9 C10 C5 -0.9(16) . . . . ?
C10 C5 C6 C7 3.8(14) . . . . ?
C11 N2 C14 C15 177.1(7) . . . . ?
C12 N2 C14 C15 56.5(9) . . . . ?
C13 N2 C14 C15 -65.9(9) . . . . ?
C14 C15 C16 C17 -178.4(9) . . . . ?
C14 C15 C20 C19 180.0(9) . . . . ?
C15 C16 C17 C18 -0.8(16) . . . . ?
C16 C15 C20 C19 3.7(14) . . . . ?
C16 C17 C18 C19 2.3(16) . . . . ?
C17 C18 C19 C20 -0.8(16) . . . . ?
C18 C19 C20 C15 -2.3(16) . . . . ?
C20 C15 C16 C17 -2.1(15) . . . . ?
C21 N3 C24 C25 178.7(7) . . . . ?
C22 N3 C24 C25 59.7(9) . . . . ?
C23 N3 C24 C25 -61.1(9) . . . . ?
C24 C25 C26 C27 -179.4(8) . . . . ?
C24 C25 C30 C29 179.2(9) . . . . ?
C25 C26 C27 C28 -0.3(14) . . . . ?
C26 C25 C30 C29 0.0(14) . . . . ?
C26 C27 C28 C29 1.1(16) . . . . ?
C27 C28 C29 C30 -1.3(17) . . . . ?
C28 C29 C30 C25 0.8(16) . . . . ?
C30 C25 C26 C27 -0.2(13) . . . . ?
C31 N4 C34 C35 177.7(8) . . . . ?
C32 N4 C34 C35 59.8(10) . . . . ?
C33 N4 C34 C35 -63.0(10) . . . . ?
C34 C35 C36 C37 180.0(9) . . . . ?
C34 C35 C40 C39 179.6(9) . . . . ?
C35 C36 C37 C38 1.8(17) . . . . ?
C36 C35 C40 C39 2.5(15) . . . . ?
C36 C37 C38 C39 -0.4(19) . . . . ?
C37 C38 C39 C40 0.0(18) . . . . ?
C38 C39 C40 C35 -1.1(16) . . . . ?
C40 C35 C36 C37 -2.8(15) . . . . ?
C41 N5 C44 C45 -173.7(9) . . . . ?
C42 N5 C44 C45 65.8(12) . . . . ?
C43 N5 C44 C45 -55.8(11) . . . . ?
C44 C45 C46 C47 -176.1(15) . . . . ?
C44 C45 C50 C49 176.8(11) . . . . ?
C45 C46 C47 C48 -3(3) . . . . ?
C46 C45 C50 C49 -2.4(19) . . . . ?
C46 C47 C48 C49 1(3) . . . . ?
C47 C48 C49 C50 -1(3) . . . . ?
C48 C49 C50 C45 1(2) . . . . ?
C50 C45 C46 C47 3(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0000 0.0000 -1.0000 0.0729 -0.0524 0.0120
1.0000 -0.0000 1.0000 -0.0729 0.0524 -0.0120
-0.0000 1.0000 -1.0000 0.0713 0.0641 0.1229
0.0000 -1.0000 1.0000 -0.0713 -0.0641 -0.1229
1.0000 0.0000 -1.0000 -0.0469 -0.0228 0.0572
-1.0000 -0.0000 1.0000 0.0469 0.0228 -0.0572
